CN108484830A - A method of both sexes drying strengthening agent is prepared using inverse emulsion polymerization - Google Patents
A method of both sexes drying strengthening agent is prepared using inverse emulsion polymerization Download PDFInfo
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- CN108484830A CN108484830A CN201810427271.3A CN201810427271A CN108484830A CN 108484830 A CN108484830 A CN 108484830A CN 201810427271 A CN201810427271 A CN 201810427271A CN 108484830 A CN108484830 A CN 108484830A
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- sexes
- emulsion polymerization
- strengthening agent
- acid
- drying strengthening
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/22—Emulsion polymerisation
- C08F2/24—Emulsion polymerisation with the aid of emulsifying agents
- C08F2/30—Emulsion polymerisation with the aid of emulsifying agents non-ionic
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
- D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
- D21H21/18—Reinforcing agents
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Paper (AREA)
Abstract
The invention discloses a kind of methods preparing both sexes drying strengthening agent using inverse emulsion polymerization, including step：Oil solvent and emulsifier are mixed, obtain mixed liquor A by step 1；Acrylamide, anionic monomer, cationic monomer, functional monomer, reaction suppressor, crosslinking agent, disodium ethylene diamine tetraacetate and water are mixed, obtain mixed liquid B by step 2；Mixed liquid B is added in mixed liquor A, emulsifies to obtain stable emulsion C by step 3；Initiator progress reverse emulsion polymerization is added into stable emulsion C, obtains both sexes drying strengthening agent after reaction for step 4.Both sexes drying strengthening agent prepared by the method for the present invention has the characteristics that low viscosity, good heat dissipation, reacts fast, molecular weight of product narrowly distributing, can increase substantially paper tensile strength, internal bond strength, while its ring crush intensity and burst index significantly improve；In addition, using the technique of inverse emulsion polymerization, exotherm in reaction process is effectively reduced, greatly reduces the generation of gel point.
Description
Technical field
The present invention relates to drying strengthening agent preparing technical fields more particularly to a kind of use inverse emulsion polymerization to prepare both sexes and do by force
The method of agent.
Background technology
China's timber resources is insufficient, and paper industry is mainly with wheat straw, reed, straw, bagasse, bamboo, cotton stalk, Chinese alpine rush etc.
Plant is raw material, and compared with timber, these raw fibres are short, intensity difference.The current paper industry in China, which is just manufactured paper with pulp by acidity, is
It unites to neutral even weak base sex reversal, is produced under high ph-values, more kinds of fillers can be used, but high filler content can make the strong of paper
Degree loss.In addition, due to the shortage of world's wooden oar, the secondary use of waste paper is gradually taken seriously, but fiber is used repeatedly
It can influence its intensity.
To sum up, at present to developing China's paper industry, it is necessary to which the development and application for reinforcing highly efficient intensifying agent are especially developed
The mating careless paddle paper making intensifier with grass fiber.And existing drying strengthening agent is not only formulated unreasonable, energy consumption height of arranging in pairs or groups, and it makes
It is undesirable with effect.
Invention content
The purpose of the present invention is the defect in the presence of for the above-mentioned prior art, propose a kind of to use inverse emulsion polymerization
The method for preparing both sexes drying strengthening agent.
To achieve the above object, the present invention uses following technical scheme：
The first aspect of the invention is to provide a kind of method preparing both sexes drying strengthening agent using inverse emulsion polymerization, including
Following steps：
Oil solvent and emulsifier are mixed, obtain mixed liquor A by step 1；
Step 2, by acrylamide, anionic monomer, cationic monomer, functional monomer, reaction suppressor, crosslinking agent,
Disodium ethylene diamine tetraacetate and water mixing, obtain mixed liquid B；
Mixed liquid B is added in mixed liquor A, emulsifies to obtain stable emulsion C by step 3；
Initiator progress reverse emulsion polymerization is added into the stable emulsion C, obtains after reaction described for step 4
Both sexes drying strengthening agent.
Further, in the method for preparing both sexes drying strengthening agent using inverse emulsion polymerization, the weight of each component
Number is as follows：
Further, the oil solvent is selected from kerosene, ortho-xylene, hexane, hexamethylene, normal heptane, isomery paraffin, different chain
One or more of alkane and gasoline.
Further, the emulsifier is selected from sorbitanmonolaureate, sorbitan mono-oleic acid ester, polyoxyethylene mountain
Pears alcohol acid anhydride monostearate, polyoxyethylene sorbitol acid anhydride list have acid esters, octadecane alcohol radical APEO, different tridecanol polyoxy second
One or more of alkene ether, benzyl dimethyl phenol polyethenoxy ether and octyl phenol polyoxyethylene ether.
Further, the cationic monomer is selected from (methyl) acryloyloxyethyl trimethyl ammonium chloride, (methyl) propylene
Sour dimethylaminoethyl, (methyl) diethylaminoethyl acrylate, diallyidimethylammonium chloride amine and dimethylamino-propyl third
One or more of acrylamide.
Further, the anionic monomer is selected from acrylic acid, methacrylic acid, itaconic acid, maleic acid, fumaric acid, horse
Come the monomers such as acid anhydrides, sodium vinyl sulfonate, vinylbenzenesulfonic acid sodium, Sodium Allyl Sulfonate and methallylsulfonic acid sodium or its salt
One or more of class.
Further, the functional monomer is selected from one or more of soft monomer, hard monomer and hydrophobic monomer.
It is further preferred that the functional monomer is selected from the light ethyl ester of acrylic acid, the light propyl ester of acrylic acid, styrene, methyl
One or more of methyl acrylate, alkyl acrylate and alkyl methacrylate.
Further, the reaction suppressor is selected from sodium hydrogensulfite, sodium pyrosulfite, sodium thiosulfate, positive 12 sulphur
One or more of alcohol, tert-dodecyl mercaptan, coloured glaze guanidine-acetic acid, coloured glaze base ethyl alcohol and isopropanol.
Further, the crosslinking agent be selected from hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide,
Diacetone Acrylamide, methylene-bisacrylamide, N, mono- diallyl acrylamides of N, N, mono- dimethacrylamide diethyls of N
One or more of alkenyl monomer and tri-vinyl monomers.
Further, the initiator is selected from potassium peroxydisulfate, ammonium persulfate, perbromic acid sodium, hydrogen peroxide, peroxidating hexamethylene
The one or more of ketone, dibenzoyl peroxide and tert-butyl hydroperoxide.
Further, the dosage of the water employed in the method for the present invention is not particularly limited, and those skilled in the art should be able to
It is adjusted according to the solid content of the dispersion mixing situation of each component, the adequacy of emulsion polymerization and final products needs；It is excellent
Choosing, the dosage of water is 50-150 parts.
It is further preferred that the reaction temperature of reverse emulsion polymerization is 50-75 DEG C in step 4, the reaction time is that 2-4 is small
When.
Further more preferably, after mixing oil solvent and emulsifier in step 1, it is heated to 45-55 DEG C, makes emulsification
Agent is completely dissolved in oil solvent；The emulsification times of step 3 are 0.1-1 hours.
The present invention is had the following technical effect that compared with prior art using above-mentioned technical proposal：
(1) preparation method of the present invention uses certain monomer ratio and reasonable process, can be made that increase substantially paper anti-
The both sexes drying strengthening agent of Zhang Qiangdu, internal bond strength, while its ring crush intensity and burst index significantly improve；
(2) both sexes drying strengthening agent prepared by the present invention has low viscosity, good heat dissipation, reaction fast, molecular weight of product narrowly distributing
Feature；
(3) technique for using inverse emulsion polymerization, effectively reduces exotherm in reaction process, greatly reduces solidifying
The generation of glue point.
Specific implementation mode
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
Embodiment 1
500 parts of kerosene, 5 parts of Span20 (sorbitanmonolaureate) are added in reaction kettle, 50 DEG C is heated to, makes
Span20 is completely dissolved in kerosene；By 80 parts of acrylamides, 10 parts of acrylic acid, 15 parts of (methyl) acrylyl oxy-ethyl-trimethyl chlorine
Change amine, 7 parts of alkyl acrylates, 0.3 part of sodium hydrogensulfite, 1 part of Diacetone Acrylamide, 0.3 part of disodium ethylene diamine tetraacetate
(EDTA-2Na) it is dissolved in suitable quantity of water and obtains certain density aqueous solution, and rapidly join in reaction kettle, continue stirring and emulsifying
After the lotion of stabilization to be obtained, a certain amount of potassium peroxydisulfate with appropriate water dissolution is added in 1h, 0.12 part of potassium peroxydisulfate dosage,
(70 DEG C) reaction 4h of constant temperature in a kettle, obtain uniform and stable polymerized emulsion product, at demulsification after reaction
After reason, solid amphoteric drying strengthening agent is obtained.
Embodiment 2
500 parts of hexanes, 5 parts of Span80 are added in reaction kettle, 50 DEG C is heated to, Span80 is made to be completely dissolved in hexane
In；By 80 parts of acrylamides, 10 parts of itaconic acids, 15 parts of (methyl) dimethylaminoethyl acrylates, 7 parts of methyl methacrylates,
0.3 part of sodium thiosulfate, 1 part of N, mono- diallyl acrylamides of N, 0.3 part of disodium ethylene diamine tetraacetate (EDTA-2Na) dissolving
Certain density aqueous solution is obtained in suitable quantity of water, and is rapidly joined in reaction kettle, and stirring and emulsifying 1h is continued, stabilization to be obtained
After lotion, a certain amount of potassium peroxydisulfate with appropriate water dissolution, 0.1 part of potassium peroxydisulfate dosage, in a kettle constant temperature (70 are added
DEG C) reaction 4h, i.e. obtain uniform and stable polymerized emulsion product obtains solid amphoteric after demulsification is handled after reaction
Drying strengthening agent.
Embodiment 3
400 parts of kerosene, 4 parts of Span20 are added in reaction kettle, 50 DEG C is heated to, Span20 is made to be completely dissolved in kerosene
In；By 64 parts of acrylamides, 8 parts of acrylic acid, 12 parts of (methyl) acryloyloxyethyl trimethyl ammonium chlorides, 5.6 parts of alkyl acrylates
Base ester, 0.25 part of sodium hydrogensulfite, 0.8 part of Diacetone Acrylamide, 0.24 part of disodium ethylene diamine tetraacetate (EDTA-2Na) are molten
Solution obtains certain density aqueous solution in suitable quantity of water, and rapidly joins in reaction kettle, continues stirring and emulsifying 1h, stabilization to be obtained
Lotion after, a certain amount of potassium peroxydisulfate with appropriate water dissolution, 0.2 part of potassium peroxydisulfate dosage, in a kettle constant temperature is added
(70 DEG C) reaction 4h, obtain uniform and stable polymerized emulsion product after reaction, after demulsification is handled, obtain solid two
Property drying strengthening agent.
Comparative example
Water 405g, acrylamide 120g, MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chloride are sequentially added in a kettle
16g, methylene-bisacrylamide 0.08g, base ethyl alcohol 1g, the light propyl ester 4g of acrylic acid, ethyl acrylate 2g and benzophenone 1g are dredged
It stirs evenly, reaction kettle is vacuumized to logical nitrogen repeatedly 2-3 times, then maintain to lead to nitrogen, temperature of reaction kettle is risen to 85 DEG C, was added
Sodium oxide molybdena, it is basic to keep reacting 1.5 hours in the case of constant temperature, start to carry out viscosity test every sampling in 20 minutes later, glue
Degree stops reaction after reaching 4500mP*S, and liquid caustic soda (32%) 1.5g is added and adjusts pH to 4-6, is eventually adding hydroquinone 0.02g,
Add water to adjust solid content to 20 scholars 1%, drying strengthening agent is made.
Application Example
1, the quantitative 150g/m that manufactures paper with pulp is designed2；
2, charging sequence is：Slurry+both sexes drying strengthening agent+APAM (300ppm)+particulate (400ppm)；
3, the additive amount of both sexes drying strengthening agent：1.6 ‰, 2.4 ‰, 3.2 ‰ (dry/dry) by 15% solid content folding 10.7,16,
21.3Kg/t paper (wet/dry)；
4, slurry is weighed, both sexes drying strengthening agent is added and stirs 2 minutes, adds APAM, particulate and respectively stirs 2 minutes, uses
After the semi-automatic sheet forming apparatus copy papers of LABTECH73-62, the squeezing of LABTECH 73-50 standard page squeezers, natural air drying,
Then quantitative, tensile strength, ring crush intensity, folding strength, internal bond strength, the bursting strength of detection paper, the result is shown in 1 institutes of table
Show：
Table 1
The both sexes drying strengthening agent prepared using the method for the present invention is can be seen that using result from above-mentioned table 1, it is strong in anti-tensile
Degree, tensile index, ring crush intensity, ring crush index, bursting strength, burst index, internal bond strength will be better than comparative example, very great Cheng
Degree improves drying strengthening agent enhancing effect, plays an important role to the secondary use of waste paper.
Specific embodiments of the present invention are described in detail above, but it is intended only as example, the present invention is simultaneously unlimited
It is formed on particular embodiments described above.To those skilled in the art, it is any to the equivalent modifications that carry out of the present invention and
It substitutes also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by impartial conversion and
Modification, all should be contained within the scope of the invention.
Claims (10)
1. a kind of method preparing both sexes drying strengthening agent using inverse emulsion polymerization, which is characterized in that include the following steps：
Oil solvent and emulsifier are mixed, obtain mixed liquor A by step 1；
Step 2, by acrylamide, anionic monomer, cationic monomer, functional monomer, reaction suppressor, crosslinking agent, second two
Amine tetraacethyl disodium and water mixing, obtain mixed liquid B；
Mixed liquid B is added in mixed liquor A, emulsifies to obtain stable emulsion C by step 3；
Initiator progress reverse emulsion polymerization is added into the stable emulsion C, obtains the both sexes after reaction for step 4
Drying strengthening agent.
2. the method according to claim 1 for preparing both sexes drying strengthening agent using inverse emulsion polymerization, which is characterized in that each group
The parts by weight divided are as follows：
3. the method according to claim 1 for preparing both sexes drying strengthening agent using inverse emulsion polymerization, which is characterized in that described
One kind in kerosene, ortho-xylene, hexane, hexamethylene, normal heptane, isomery paraffin, isoparaffin and gasoline of oil solvent or
It is several；It is stearic that the emulsifier is selected from sorbitanmonolaureate, sorbitan mono-oleic acid ester, polyoxyethylene sorbitol acid anhydride list
Acid esters, polyoxyethylene sorbitol acid anhydride list have acid esters, octadecane alcohol radical APEO, different tridecanol polyoxyethylene ether, benzyl two
One or more of methyl phenol polyethenoxy ether and octyl phenol polyoxyethylene ether.
4. the method according to claim 1 for preparing both sexes drying strengthening agent using inverse emulsion polymerization, which is characterized in that described
Cationic monomer is selected from (methyl) acryloyloxyethyl trimethyl ammonium chloride, (methyl) dimethylaminoethyl acrylate, (methyl)
One or more of diethylaminoethyl acrylate, diallyidimethylammonium chloride amine and dimethylamino propyl acrylamide；
The anionic monomer is selected from acrylic acid, methacrylic acid, itaconic acid, maleic acid, fumaric acid, maleic anhydride, vinyl sulfonic acid
One or more of the monomers or its esters such as sodium, vinylbenzenesulfonic acid sodium, Sodium Allyl Sulfonate and methallylsulfonic acid sodium.
5. the method according to claim 1 for preparing both sexes drying strengthening agent using inverse emulsion polymerization, which is characterized in that described
Functional monomer is selected from one or more of soft monomer, hard monomer and hydrophobic monomer.
6. the method according to claim 5 for preparing both sexes drying strengthening agent using inverse emulsion polymerization, which is characterized in that described
Functional monomer be selected from the light ethyl ester of acrylic acid, the light propyl ester of acrylic acid, styrene, methyl methacrylate, alkyl acrylate and
One or more of alkyl methacrylate.
7. the method according to claim 1 for preparing both sexes drying strengthening agent using inverse emulsion polymerization, which is characterized in that described
Reaction suppressor is selected from sodium hydrogensulfite, sodium pyrosulfite, sodium thiosulfate, n- dodecyl mereaptan, tert-dodecyl mercaptan, coloured glaze base second
One or more of acid, coloured glaze base ethyl alcohol and isopropanol.
8. the method according to claim 1 for preparing both sexes drying strengthening agent using inverse emulsion polymerization, which is characterized in that described
Crosslinking agent is selected from hydroxy propyl methacrylate, divinylbenzene, N hydroxymethyl acrylamide, Diacetone Acrylamide, methylene
Bisacrylamide, N, mono- diallyl acrylamides of N, N, mono- dimethacrylamide di-vinyl monomers of N and trivinyl list
One or more of body；The initiator is selected from potassium peroxydisulfate, ammonium persulfate, perbromic acid sodium, hydrogen peroxide, peroxidating hexamethylene
One or more of ketone, dibenzoyl peroxide and tert-butyl hydroperoxide.
9. according to the method that claim 1-8 any one of them prepares both sexes drying strengthening agent using inverse emulsion polymerization, feature
It is, the reaction temperature of reverse emulsion polymerization is 50-75 DEG C in step 4, and the reaction time is 2-4 hours.
10. the method according to claim 9 for preparing both sexes drying strengthening agent using inverse emulsion polymerization, which is characterized in that step
After mixing oil solvent and emulsifier in rapid one, it is heated to 45-55 DEG C, emulsifier is made to be completely dissolved in oil solvent；Step 3
Emulsification times are 0.1-1 hours.
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| CN201810427271.3A CN108484830A (en) | 2018-05-07 | 2018-05-07 | A method of both sexes drying strengthening agent is prepared using inverse emulsion polymerization |
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| CN201810427271.3A CN108484830A (en) | 2018-05-07 | 2018-05-07 | A method of both sexes drying strengthening agent is prepared using inverse emulsion polymerization |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024089994A1 (en) * | 2022-10-25 | 2024-05-02 | ハイモ株式会社 | Water droplet-in-oil emulsion paper strength enhancer |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101403204A (en) * | 2008-10-07 | 2009-04-08 | 杭州杭化播磨造纸化学品有限公司 | Surface sizing agent for amphiprotic papermaking and its preparation method |
| CN103788315A (en) * | 2014-01-15 | 2014-05-14 | 江苏富淼科技股份有限公司 | Preparation method for amphoteric water-in-oil inverse emulsion |
-
2018
- 2018-05-07 CN CN201810427271.3A patent/CN108484830A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101403204A (en) * | 2008-10-07 | 2009-04-08 | 杭州杭化播磨造纸化学品有限公司 | Surface sizing agent for amphiprotic papermaking and its preparation method |
| CN103788315A (en) * | 2014-01-15 | 2014-05-14 | 江苏富淼科技股份有限公司 | Preparation method for amphoteric water-in-oil inverse emulsion |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024089994A1 (en) * | 2022-10-25 | 2024-05-02 | ハイモ株式会社 | Water droplet-in-oil emulsion paper strength enhancer |
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